CN111533232A - Precipitated lithium tail liquid carbon removal device and system - Google Patents

Precipitated lithium tail liquid carbon removal device and system Download PDF

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Publication number
CN111533232A
CN111533232A CN202010250258.2A CN202010250258A CN111533232A CN 111533232 A CN111533232 A CN 111533232A CN 202010250258 A CN202010250258 A CN 202010250258A CN 111533232 A CN111533232 A CN 111533232A
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lithium
hydrochloric acid
liquid
reaction vessel
tail liquid
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CN202010250258.2A
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CN111533232B (en
Inventor
何永平
孙海东
张成胜
严雄仲
宋爱清
白顺梅
谈广德
孙海新
昝仁鹏
运建月
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Qinghai Salt Lake Industry Co Ltd
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Qinghai Salt Lake Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a device and a system for removing carbon from lithium precipitation tail liquid. The lithium precipitation tail liquid decarbonization device comprises a lithium precipitation tail liquid pump 9, a hydrochloric acid pump 8, a reaction container 4 and a pH value on-line monitoring analyzer 19. The hydrochloric acid pump is connected to a hydrochloric acid injection coil 5 disposed within the reaction vessel. The lithium tailing pump is connected to a lithium precipitation tailing spray pipe 12a provided in the reaction vessel. The reaction vessel 4 is connected to a main mother liquor discharge pipe 28. The pH value on-line monitoring analyzer 19 is mounted on the reaction vessel to monitor the pH value of the liquid in the reaction vessel. The reaction vessel 4 is provided with a level gauge 14. The lithium precipitation tail liquid is mixed with hydrochloric acid in the reaction vessel 4, and sodium carbonate in the lithium precipitation tail liquid is removed by reaction with the hydrochloric acid. Compared with the mixing reaction of the lithium precipitation tail liquid and hydrochloric acid in a tedding salt pan or a neutralization stirring tank, the method can automatically remove carbon, prevent unqualified mother liquid quality caused by overhigh or overlow pH value of the mother liquid and the like, and more effectively extract lithium resources from the lithium precipitation tail liquid.

Description

Precipitated lithium tail liquid carbon removal device and system
Technical Field
The invention relates to the technical field of lithium carbonate production by an adsorption method, in particular to a device and a system for removing carbon from lithium precipitation tail liquid.
Background
At present, lithium carbonate is mainly produced by an electrodialysis method, an extraction method, a calcination method, a precipitation method, an adsorption method and the like in China. The lithium resource required for production is possessed in the salt lake brine of the Cheddar basin, and the magnesium-lithium ratio of the salt lake brine is about 500: 1. Under the restriction of the factor of the ultrahigh magnesium-lithium ratio, the extraction of lithium resources by adopting the electrodialysis method, the extraction method, the calcination method, the precipitation method and the like which are commonly used in China is difficult, and the lithium extraction technology by using the ion resin exchange adsorption method is needed to produce the lithium carbonate.
The main process is that old bittern (magnesium-lithium ratio 500: 1) discharged from potash fertilizer production is pumped into an adsorption tower filled with lithium selective adsorption resin for adsorption, and tail bittern is discharged. After the adsorption saturation, a lithium washing process is adopted to wash out magnesium chloride carried in the bed layer, and then the qualified lithium chloride solution (qualified solution for short) is obtained by leaching. And deeply removing magnesium, concentrating and separating the qualified liquid, and then reacting the qualified liquid with a sodium carbonate solution to prepare lithium carbonate. In the process, qualified liquid generates a large amount of lithium precipitating tail liquid (the lithium content is higher than lithium forming brine) when passing through the working procedures of washing and filtering, pulp preparation and washing and centrifugal separation of a vacuum horizontal belt filter, and the lithium precipitating tail liquid is directly discharged into an impermeable salt field to be spread, evaporated, concentrated and decarbonized for reuse.
The existing decarbonization method is to add acid directly in the salt pan or stir and mix two media in a neutralization tank for neutralization through a stirrer, the two methods have the condition that the pH value is not easy to control due to uneven mixing reaction in use, so that the quality of the salt pan mother liquor is unqualified, the salt pan mother liquor is conveyed to a subsequent production system through a pump to cause serious influence on subsequent production, the product quality and production are influenced, and great economic loss is caused.
Therefore, a tool capable of efficiently removing carbon in lithium precipitation tail liquid recovery in lithium carbonate production is needed.
Disclosure of Invention
The invention aims to provide a decarbonization device and a decarbonization system for treating lithium precipitation tail liquid to replace decarbonization carried out in a salt pan.
The first technical scheme is a lithium-precipitating tail liquid carbon removal device which is characterized by comprising a lithium-precipitating tail liquid pump (9), a hydrochloric acid pump (8) and a reaction container (4); the reaction vessel (4) is of a cylindrical structure with a bottom, the top of the reaction vessel is sealed by a top cover (16),
the hydrochloric acid pump (8) is connected with a hydrochloric acid spraying coil pipe (5) arranged in the reaction vessel (4) through a pipeline (12), and the lithium precipitation tailing pump (9) is connected with a lithium precipitation tailing liquid spraying pipe (12a) arranged in the reaction vessel (4) through a pipeline (3);
a mother liquor discharge port (21) is formed in the bottom of the side wall of the reaction container (4), the mother liquor discharge port (21) is connected with a main mother liquor discharge pipe (28) through a pipeline, and a control valve (23) is arranged on the pipeline connected with the mother liquor discharge port (21);
the hydrochloric acid injection coil (5) is spirally arranged on the inner wall of the reaction container (4) around the circumference of the reaction container (4), the pipe wall of the hydrochloric acid injection coil (5) facing the center of the reaction container (4) is provided with an injection hole (7),
preferably, on the hydrochloric acid injection coil (5), the aperture of the injection hole (7) positioned on the upper section and the lower section of the hydrochloric acid injection coil (5) is larger than that of the injection hole (7) positioned on the middle section of the hydrochloric acid injection coil (5).
Preferably, the lithium deposition tail liquid inlet pipe (12a) comprises a first straight pipe section, an elbow and a second straight pipe section, and the first straight pipe section is connected with the second straight pipe section through the elbow.
Preferably, the included angle between the first straight pipe section and the second straight pipe section is 90 degrees, and the center line of the first straight pipe section and the center line of the second straight pipe section are perpendicular to the center line of the reaction vessel (4).
Preferably, a first lithium precipitation tail liquid inlet hole (2u) and a second lithium precipitation tail liquid inlet hole (2d) which are connected with the pipeline (3) and a hydrochloric acid inlet hole (3a) which is connected with the pipeline (12) are arranged on the side wall of the reaction vessel (4);
the first lithium precipitation tail liquid inlet hole (2u) and the second lithium precipitation tail liquid inlet hole (2d) are arranged at positions close to the top cover (16) and the reaction container (4), the hydrochloric acid inlet hole (3a) is arranged at a position between the first lithium precipitation tail liquid inlet hole (2u) and the second lithium precipitation tail liquid inlet hole (2d), and the side surface of the hydrochloric acid inlet hole is located in the region of the hydrochloric acid spraying coil pipe (5).
Preferably, the device also comprises an ultrasonic liquid level meter (5) and a displacement type liquid level meter (18), wherein the ultrasonic liquid level meter (5) is arranged at the top of the reaction vessel (4), and the displacement type liquid level meter (18) is arranged on the side wall of the reaction vessel (4).
Preferably, a control ball valve (1b) and a check valve (11) are sequentially arranged on the pipeline (12) along the liquid outlet direction of the hydrochloric acid pump (8),
a control ball valve (2b) and a check valve (11) are sequentially arranged on the pipeline (3) along the liquid outlet direction of the lithium precipitation tailing pump (9),
preferably, a vent pipe (15) communicated with the inside of the reaction vessel (4) is arranged on a top cover (16) of the reaction vessel (4).
Preferably, both ends of the displacement type liquid level meter 18 are closed, a lower interface of the displacement type liquid level meter 18 is communicated with the inside of the reaction vessel 4 through a liquid level meter control valve 24d, and an upper interface of the displacement type liquid level meter 18 is communicated with the inside of the reaction vessel 4 through a liquid level meter control valve 24 u.
The second technical scheme is a lithium precipitation tail liquid carbon removal system which is characterized by comprising a distributed controller (30), an ultrasonic liquid level meter (14), a pH value on-line monitoring analyzer (19) and a lithium precipitation tail liquid carbon removal device,
the ultrasonic liquid level meter (14) monitors the liquid level of a reaction container in the lithium precipitation tail liquid decarbonization device, the pH value on-line monitoring analyzer (19) monitors the pH value of liquid in the reaction container in the lithium precipitation tail liquid decarbonization device,
the distributed controller (30) controls the lithium precipitation tailing pump (9) and the hydrochloric acid pump (8) according to the liquid level monitored by the ultrasonic liquid level meter (14) and the pH value monitored by the pH value on-line monitoring analyzer (19),
the lithium precipitating tail liquid device is the lithium precipitating tail liquid carbon removal device as claimed in any one of claims 1-9.
Drawings
FIG. 1 is a schematic structural diagram of a lithium precipitation tail liquid decarbonization device provided by the present invention;
FIG. 2 is a schematic sectional view of a horizontal plane of a reaction vessel of the device for removing carbon from the lithium precipitating tail solution provided by the present invention;
fig. 3 is an explanatory diagram of a distributed control system in the lithium precipitating tail liquid decarbonization system provided by the invention.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention more clear, the technical solutions of the present invention are further described below with reference to the accompanying drawings and the detailed description. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
As shown in FIG. 1, the device for removing carbon from the lithium precipitation tail liquid of the invention is composed of a reaction vessel 4 and peripheral components. The reaction vessel 4 is a round reaction kettle with a bottom cylindrical structure, the top of the reaction vessel is provided with a top cover 16, the top cover 16 is fixed on the top cylinder opening of the reaction vessel 4 by a bolt 17, and the top cover and the top cylinder opening are sealed by a sealing ring 13 to form a closed cavity. A top cover 16 of the reaction vessel 4 is provided with a vent pipe 15 communicating with the inside of the reaction vessel 4.
The reaction vessel 4 is provided with a hydrochloric acid injection coil 5 inside. The hydrochloric acid spraying coil pipe 5 is formed in a spiral shape, has a uniform interval between turns, and is fixed to the inner wall of the reaction vessel 4 by a fixing clip 6 (see fig. 2).
A first lithium precipitation tail liquid inlet hole 2u, a hydrochloric acid inlet hole 3a and a second lithium precipitation tail liquid inlet hole 2d are formed in sequence from top to bottom on the side wall of the reaction vessel 4. When seen from the side surfaces of the first lithium precipitation tail liquid inlet hole 2u, the hydrochloric acid inlet hole 3a and the second lithium precipitation tail liquid inlet hole 2d, the first lithium precipitation tail liquid inlet hole, the hydrochloric acid inlet hole and the second lithium precipitation tail liquid inlet hole are positioned in the area of the hydrochloric acid spraying coil pipe 5. The hydrochloric acid liquid inlet hole 3a is positioned in the middle of the hydrochloric acid spraying coil pipe 5 and is communicated with the hydrochloric acid spraying coil pipe 5.
The first lithium precipitation tail liquid inlet hole 2u and the second lithium precipitation tail liquid inlet hole 2d are adjacent to the uppermost end and the lowermost end of the hydrochloric acid spraying coil pipe 5, and a lithium precipitation tail liquid inlet pipe 12a which is respectively communicated with the first lithium precipitation tail liquid inlet hole 2u and the second lithium precipitation tail liquid inlet hole 2d is arranged inside the reaction vessel 4. Except that the two lithium deposition tail liquid inlet pipes 12a are arranged at different positions, the rest are the same, and the lithium deposition tail liquid inlet pipe 12a communicated with the first lithium deposition tail liquid inlet hole 2u is explained below.
As shown in fig. 2, the lithium precipitating tail liquid inlet pipe 12a is composed of a first straight pipe section, an elbow and a second straight pipe section which are communicated with the first lithium precipitating tail liquid inlet hole 2 u. The first straight pipe section and the second straight pipe section are in fluid conduction connection through the elbow, and the included angle between the first straight pipe section and the second straight pipe section is 90 degrees. The central line of the first straight pipe section and the central line of the second straight pipe section are vertical to the central line of the reaction vessel 4, and the second straight pipe section is used as a liquid outlet and sprays lithium deposition tail liquid along the inner wall of the reaction vessel 4. The second straight pipe section as the liquid outlet is positioned at the inner side (close to the center of the reaction vessel) of the hydrochloric acid spraying coil pipe 5, and the lithium deposition tail liquid sprayed by the second straight pipe section is intersected with the hydrochloric acid sprayed by the hydrochloric acid spraying coil pipe 5.
The spraying directions of the lithium tail liquid inlet pipe 12a of the first lithium tail liquid inlet hole 2u and the lithium tail liquid inlet pipe 12a of the second lithium tail liquid inlet hole 2d are the same. In the present embodiment, the lithium deposition solutions are ejected counterclockwise along the inner wall of the reaction vessel 4.
The two ends of the hydrochloric acid injection coil pipe 5 are closed, and the pipe wall is provided with an injection hole 7. As shown in fig. 2, the injection holes 7 face toward the center line of the reaction vessel 4, and the center line of the injection holes 7 is perpendicular to the center line of the reaction vessel 4. The spray holes 7 located on the upper (about 1/3 for the entire coil) and lower (about 1/3 for the entire coil) sections of the hydrochloric acid spray coil 5 are larger in aperture than the spray holes 7 located on the middle (about 1/3 for the entire coil) section of the hydrochloric acid spray coil 5. Make each jet orifice of whole hydrochloric acid injection coil 5 can jet out the roughly the same hydrochloric acid of flow, promptly, hydrochloric acid injection coil 5 middle section is because being close to hydrochloric acid feed liquor hole 3a, and the pressure is bigger than hydrochloric acid injection coil 5 upper segment and hypomere, and the aperture sets up to be less relatively, has guaranteed that each jet orifice 7 of whole hydrochloric acid injection coil 5 sprays the roughly the same flow.
The liquid outlet end of the hydrochloric acid pump 8 is connected with a pipeline 12, and the other end of the pipeline 12 is connected with a hydrochloric acid liquid inlet hole 3a through a flange and communicated with a hydrochloric acid injection pipe 5 arranged in the reaction vessel 4.
A pressure gauge 10, a control ball valve 1b and a check valve 11 are sequentially arranged on a pipeline 12 at the liquid outlet end of the hydrochloric acid pump 8 along the liquid outlet direction of the hydrochloric acid pump 8.
The liquid outlet end of the lithium precipitation tail liquid pump 9 is connected with the pipeline 3, and the other end of the pipeline 3 is respectively connected with the first lithium precipitation tail liquid inlet hole 2u and the second lithium precipitation tail liquid inlet hole 2d through flanges and is communicated with a lithium precipitation tail liquid inlet pipe 12a in the reaction vessel 4.
A pressure gauge 10, a control ball valve 2b and a check valve 11 are sequentially arranged on the pipeline 3 at the liquid outlet end of the lithium precipitation tail liquid pump 9 along the liquid outlet direction of the lithium precipitation tail liquid pump 9.
The liquid inlet ends of the hydrochloric acid pump 8 and the lithium precipitation tail liquid pump 9 are respectively provided with a control ball valve 1a and a control ball valve 1 b.
The side wall of the reaction vessel 4 is positioned at the bottom and is provided with a mother liquor outlet 21, the mother liquor outlet 21 is communicated with a main mother liquor outlet 28 through a flange, and a pipeline communicated with the main mother liquor outlet 28 is provided with a control valve 23.
The side wall of the reaction vessel 4 is provided at the top with an overflow hole 26 communicating with the inside of the reaction vessel 4. The overflow pipe 20 is connected to an overflow hole 26 via a flange, the other end of the overflow pipe 20 communicates with a main mother liquor discharge pipe 28, and a control valve 22 is provided in the piping of the overflow pipe 20.
The overflow hole 26 is located at a high level above the hydrochloric acid injection coil 5, i.e. at the level of point a in fig. 1 (acceptable level).
A displacement type level gauge 18 is attached to the side wall of the reaction vessel 4, and both ends of the displacement type level gauge 18 are closed. The lower port of the displacement type gauge 18 communicates with a lower gauge through-hole provided in the side wall of the reaction vessel 4 through a gauge control valve 24 d. The lower level meter through hole is arranged at the position which is a little higher than the mother liquor discharge port 21 at the bottom of the side wall of the reaction vessel 4, and the upper interface of the displacement type level meter 18 is communicated with the inner part of the reaction vessel 4 through a level meter control valve 24u and an upper level meter through hole 25 arranged at the top of the reaction vessel 4. The upper gauge through hole 25 is slightly higher than the position of the overflow hole 26, i.e. at the level of point B in fig. 1.
Because the upper end of the displacement type liquid level meter 18 is communicated with the inside of the reaction vessel 4, compared with a liquid level meter with an opening at the upper end, the liquid in the reaction vessel 4 can not be communicated with the outside through the displacement type liquid level meter 18, and the operation environment is protected.
The reaction vessel 4 is provided with a drain port 27 at the bottom center thereof. The drain pipe is connected with a drain port 27 through a flange, and the other end of the drain pipe is communicated with a main mother liquor discharge pipe 28. The drain pipe is provided with a drain valve 29 on the pipeline.
An ultrasonic level gauge 14 is installed at the center of a top cover 16 of the reaction vessel 4. An on-line pH value monitoring analyzer 19 is arranged in the middle of the side wall of the reaction vessel 4.
Examples
In the present embodiment, the reaction vessel 4 has a diameter of 3m and a height of 4 m.
The aperture of the injection hole 7 on the upper section and the lower section is 6-8 mm, the aperture of the injection hole 7 on the middle section is 4-6 mm, and the distance between two adjacent injection holes 7 is 10-15 cm. The aperture is 4-6 mm, and the distance between two adjacent jet holes 7 on the same 5 pipe sections of the hydrochloric acid jet coil is 10-15 cm.
The distance between the liquid inlet hole 2u of the first lithium precipitation tail liquid and the bottom of the reaction vessel 4 is 2.9 m; the distance between the liquid inlet hole 2d of the second lithium precipitation tail liquid and the bottom of the reaction vessel 4 is 0.9 m; the hydrochloric acid liquid inlet hole 3a arranged in the middle of the reaction vessel 4 is 1.9m away from the bottom of the reaction vessel 4. The distance between the lowest plate of the hydrochloric acid spraying coil pipe 5 and the bottom of the reaction vessel 4 is 5-8 cm, the distance between the uppermost plate of the hydrochloric acid spraying coil pipe 5 and the lower line of the qualified liquid level is 5-8 cm, and the qualified liquid level (A in the figure 1) is 3.6m (inclusive) to 3.8m (exclusive).
A mother liquor discharge port 21 is provided below the lowermost tray of the hydrochloric acid spraying coil 5.
The lithium precipitation tail liquid carbon removal system is composed of a lithium precipitation tail liquid carbon removal device and a distributed controller.
Fig. 3 is an explanatory diagram of a distributed controller in the lithium precipitating tail liquid decarbonization system provided by the invention.
As shown in fig. 3, a Distributed Controller (DCS)30 is connected to a pH value online monitoring analyzer 19, a pressure gauge 10(10a) on the pipeline 12, a pressure gauge 10(10b) on the pipeline 3, an ultrasonic level meter 14, a hydrochloric acid pump 8, a lithium precipitation tail liquid pump 9, a control ball valve 23, and a control ball valve 22.
When the precipitated lithium tail liquid decarbonization system is used for decarbonizing the precipitated lithium tail liquid, the control ball valves 1a and 1b are opened firstly. And remotely starting a lithium precipitation tail liquid pump 9 by a Distributed Controller (DCS)30, and pumping the lithium precipitation tail liquid into the reaction container 4. The lithium deposition tail liquid is sprayed out along the side wall of the reaction vessel 4 in the horizontal direction by the lithium deposition tail liquid inlet pipe 12a, and rotates along the side wall of the reaction vessel 4 in the counterclockwise direction.
And when the liquid level in the reaction container 4 rises to be 3m away from the bottom of the reaction container 4, the distributed controller 30 starts the hydrochloric acid pump 8, the hydrochloric acid is pumped into the reaction container 4 and is sprayed into the reaction container 4 through the hydrochloric acid spraying coil 5, the hydrochloric acid is fully mixed with the lithium precipitation tail liquid rotating anticlockwise in the reaction container 4, the mixture reacts with the sodium carbonate in the lithium precipitation tail liquid, and the sodium carbonate component in the lithium precipitation tail liquid is removed. And when the liquid level in the reaction container 4 continuously rises to the lower limit of the qualified liquid level of 3.6m, controlling the flow of the hydrochloric acid pump 8 in real time according to the pH value of the solution in the reaction container 4 monitored by the pH value on-line monitoring analyzer 19, so that the pH value of the mixed solution in the reaction container 4 is within the range of 5.8-7.2. Therefore, the pH value of the mixed solution in the reaction vessel 4 is always within the normal range of 5.8-7.2 under the normal operation state and the specified conditions.
The distributed controller 30 opens the control valve 23 arranged in the main mother liquor discharge pipe 28 on the reaction vessel 4, and the treated lithium deposition tail liquid is conveyed to the tedding salt pan through the main mother liquor discharge pipe 28. The liquid discharge speed through the control valve 23 is less than the pumping speed of the lithium deposition tail liquid by the lithium deposition tail liquid pump 9.
Because the lithium-precipitating tail liquid is rich in lithium, and after carbon removal, the lithium-precipitating tail liquid can be directly used as a raw material for extracting lithium after tedding, evaporation and concentration in a salt pan.
When the liquid level in the reaction vessel 4 rises to the acceptable liquid level of 3.7m, that is, the liquid level is at the position shown by the point A in FIG. 1, the distributed controller 30 opens the control ball valve 22 provided in the overflow pipe 20 based on the detection value of the ultrasonic level meter 14, and the overflow pipe 20 starts to discharge liquid, and is in a steady state. The control ball valve 22 may also be pre-opened. That is, in the present embodiment, since the total amount of the lithium deposition tail liquid obtained by pressurizing the reaction vessel 4 by the hydrochloric acid pump 8 and the lithium deposition tail liquid pump 9 is less than the sum of the flow rate of the mother liquid main discharge pipe 28 and the flow rate of the overflow pipe 20 at normal pressure, the amount of the lithium deposition tail liquid is balanced, and the liquid level is maintained at the height of the point a (acceptable liquid level) where the overflow hole 26 is located.
When the system is stopped, the distributed controller 30 stops the lithium precipitation tail liquid pump 9 and the hydrochloric acid pump 8, and according to the detection value of the ultrasonic liquid level meter 14, when the liquid level in the reaction container 4 is reduced to a low liquid level, namely the displacement type liquid level meter 18 displays 0.1m, the control valve 23 on the mother liquid main discharge pipe 28 is closed, and the system stops running. If the reaction vessel 4 needs to be overhauled, the drain valve 29 at the bottom of the reaction vessel 4 is opened to drain the solution in the reaction vessel 4 and the solution is qualified after replacement. And the top cover of the reaction vessel 4 is opened for maintenance after other maintenance conditions are met.
When the mother liquor main discharge pipe 28 is blocked or other accidents happen, when the detected liquid level of the ultrasonic liquid level meter 14 reaches a high liquid level of 3.8m, namely when the liquid level reaches the position shown by the point B in figure 1, the distributed controller 30 stops the hydrochloric acid pump 8 and the lithium precipitation tail liquid pump 9, so that the system enters an automatic shutdown state and performs automatic liquid discharge through the overflow pipe 20 and the mother liquor main discharge pipe 28.
In this embodiment, the distributed controller 30 performs the control of the hydrochloric acid pump 8 and the lithium deposition tail liquid pump 9 on the control valves 23 by means of the existing DCS programming.
The invention has the beneficial effects that:
1. through the processing of lithium tail liquid decarbonization system that sinks, can effectively prevent to sink lithium tail liquid and hydrochloric acid and can make and sink lithium tail liquid and hydrochloric acid reaction complete because of sinking lithium tail liquid can not fully mix in tedding salt pan or neutralization agitator tank, avoid the mother liquor because of the PH value is too high or low and the mother liquor because of the unqualified condition that causes serious influence to production takes place.
2. The method has the advantages that carbonate ions in the salt pan mother liquor are sufficiently removed, the problems that manual direct acidification causes equipment failure, damage and uneven and insufficient neutralization of materials and causes unqualified mother liquor treatment are solved, the problems that manual direct acidification causes equipment failure, damage and uneven and insufficient neutralization of materials and causes unqualified mother liquor treatment and affects subsequent normal production are solved, and the method is simple to manufacture, low in investment, convenient to install, fast, good in use effect and the like.
3. The method has the advantages that the number of operators is reduced, the danger of acid and alkali to staff is reduced, the accuracy of controlling the pH value of the salt pan mother liquor is improved, the labor and material cost of an enterprise is reduced, the production cost is reduced, the safety of the staff is improved, and large economic benefits and personnel safety guarantee are brought to the enterprise with small investment.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes and substitutions that can be easily made by those skilled in the art within the technical scope of the present invention described above should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. The device for removing carbon from the lithium precipitation tail liquid is characterized by comprising a lithium precipitation tail liquid pump (9), a hydrochloric acid pump (8) and a reaction container (4); the reaction vessel (4) is of a cylindrical structure with a bottom, the top of the reaction vessel is sealed by a top cover (16),
the hydrochloric acid pump (8) is connected with a hydrochloric acid spraying coil pipe (5) arranged in the reaction vessel (4) through a pipeline (12), and the lithium precipitation tailing pump (9) is connected with a lithium precipitation tailing liquid spraying pipe (12a) arranged in the reaction vessel (4) through a pipeline (3);
a mother liquor discharge port (21) is formed in the bottom of the side wall of the reaction container (4), the mother liquor discharge port (21) is connected with a main mother liquor discharge pipe (28) through a pipeline, and a control valve (23) is arranged on the pipeline connected with the mother liquor discharge port (21);
the hydrochloric acid injection coil (5) is spirally installed on the inner wall of the reaction container (4) around the circumference of the reaction container (4), and a jet hole (7) is formed in the pipe wall of the hydrochloric acid injection coil (5) facing the center of the reaction container (4).
2. The lithium precipitating tail liquid carbon removal device according to claim 1, wherein the aperture of the spray holes (7) on the upper section and the lower section of the hydrochloric acid spray coil (5) on the hydrochloric acid spray coil (5) is larger than that of the spray holes (7) on the middle section of the hydrochloric acid spray coil (5).
3. The lithium precipitating tail liquid carbon removal device according to claim 1, wherein the lithium precipitating tail liquid inlet pipe (12a) comprises a first straight pipe section, an elbow and a second straight pipe section, and the first straight pipe section and the second straight pipe section are connected through the elbow.
4. The lithium precipitating tail liquid carbon removal device according to claim 3, wherein the included angle between the first straight pipe section and the second straight pipe section is 90 degrees, and the center line of the first straight pipe section and the center line of the second straight pipe section are perpendicular to the center line of the reaction vessel (4).
5. The lithium precipitating tail liquid decarbonization device according to any one of claims 1 to 5, characterized in that a first lithium precipitating tail liquid inlet hole (2u) and a second lithium precipitating tail liquid inlet hole (2d) connected with the pipeline (3), and a hydrochloric acid inlet hole (3a) connected with the pipeline (12) are arranged on the side wall of the reaction vessel (4);
the first lithium precipitation tail liquid inlet hole (2u) and the second lithium precipitation tail liquid inlet hole (2d) are arranged at positions close to the top cover (16) and the reaction container (4), the hydrochloric acid inlet hole (3a) is arranged at a position between the first lithium precipitation tail liquid inlet hole (2u) and the second lithium precipitation tail liquid inlet hole (2d), and the side surface of the hydrochloric acid inlet hole is located in the region of the hydrochloric acid spraying coil pipe (5).
6. The lithium precipitation tail liquid carbon removal device according to any one of claims 1 to 5, further comprising an ultrasonic liquid level meter (5) and a displacement type liquid level meter (18), wherein the ultrasonic liquid level meter (5) is installed at the top of the reaction vessel (4), and the displacement type liquid level meter (18) is installed on the side wall of the reaction vessel (4).
7. The device for removing carbon from the lithium precipitating tail solution according to any one of claims 1 to 5,
a control ball valve (1b) and a check valve (11) are sequentially arranged on the pipeline (12) along the liquid outlet direction of the hydrochloric acid pump (8),
and a control ball valve (2b) and a check valve (11) are sequentially arranged on the pipeline (3) along the liquid outlet direction of the lithium precipitation tailing pump (9).
8. The device for removing carbon from the lithium precipitating tail solution according to any one of claims 1 to 5,
and a vent pipe (15) communicated with the inside of the reaction container (4) is arranged on a top cover (16) of the reaction container (4).
9. The device for removing carbon from the lithium precipitating tail solution according to any one of claims 1 to 5,
the both ends of displacement type level gauge 18 are sealed, the lower interface of displacement type level gauge (18) passes through level gauge control valve (24d) and sets up at reaction vessel 4 inside intercommunication, the last interface of displacement type level gauge (18) passes through level gauge control valve (24u) and sets up the inside intercommunication with reaction vessel (4).
10. A carbon removal system for lithium precipitation tail liquid is characterized by comprising a distributed controller (30), an ultrasonic liquid level meter (14), a pH value on-line monitoring analyzer (19) and a carbon removal device for lithium precipitation tail liquid,
the ultrasonic liquid level meter (14) monitors the liquid level of a reaction container in the lithium precipitation tail liquid decarbonization device, the pH value on-line monitoring analyzer (19) monitors the pH value of liquid in the reaction container in the lithium precipitation tail liquid decarbonization device,
the distributed controller (30) controls the lithium precipitation tailing pump (9) and the hydrochloric acid pump (8) according to the liquid level monitored by the ultrasonic liquid level meter (14) and the pH value monitored by the pH value on-line monitoring analyzer (19),
the lithium precipitating tail liquid device is the lithium precipitating tail liquid carbon removal device as claimed in any one of claims 1-9.
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CN105347364A (en) * 2015-10-30 2016-02-24 华陆工程科技有限责任公司 Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production
CN107835576A (en) * 2017-11-17 2018-03-23 奥士康科技股份有限公司 A kind of automatic solution adding system
CN207243639U (en) * 2017-08-08 2018-04-17 天津泰达环保有限公司 A kind of sewage-treatment plant

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Publication number Priority date Publication date Assignee Title
CN1781847A (en) * 2004-11-24 2006-06-07 中国石化集团巴陵石油化工有限责任公司 Process for producing lithium chloride using waste liquid containing lithium
US20130313199A1 (en) * 2012-05-23 2013-11-28 High Sierra Energy, LP System and method for treatment of produced waters
CN105347364A (en) * 2015-10-30 2016-02-24 华陆工程科技有限责任公司 Method for closed-loop recycling of lithium precipitation mother liquor in lithium carbonate production
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